Led packaging material and manufacturing method of the same

ABSTRACT

A light-emitting diode (LED) packaging material is formed by compounding graphene with silane or epoxy resin, to improve the defects of manufacturing an LED packaging material only of silane or epoxy resin. The addition of graphene helps improve the performance of the LED packaging material. Also provided is a manufacturing method of a LED packaging material.

This is a continuation application of copending U.S. patent applicationSer. No. 15/737,159 filed on Dec. 15, 2017, which is a national stage ofPCT Application No. PCT/CN2017/087821, filed on Jun. 9, 2017, claimingforeign priority of Chinese Patent Application No. 201710334882.9 filedon May 12, 2017, entitled “LED Packaging Material and ManufacturingMethod of the same”, which is incorporated by reference in its entirety.

BACKGROUND OF THE INVENTION Field of Invention

The present invention relates to a light-emitting diode (LED) packagingmaterial, and more particularly to a LED packaging material withgraphene and a manufacturing method of the same.

Description of Prior Art

LED is constituted of chips, metal wires, brackets, conductive plastic,packaging materials, and etc., and the main function of the packagingmaterial is to seal for preventing the chips from affecting by humidity,temperature, and oxidation, to reduce the efficiency, thus protectingthe normal operation of the chips. In addition, the packaging materialalso has the following functions: fix electronic devices to avoidchanges of the device parameters on the electronic devices due to impactof mechanical vibration and etc.; reduce the refractive index betweenLED chips and air to improve light emission efficiency; and play acooling function for the LED chips. Therefore, the LED packagingmaterial not only has a better sealing, a high transmittance, but alsohas a better bonding strength. The conventional LED packaging materialsare mainly an epoxy resin, a silicone and other materials. Among them,the epoxy resin is for its excellent adhesion, electrical insulation,sealing and dielectric properties and the cost is relatively low, easyto shape and other characteristics to become a mainstream material of aLED packaging. The silicone material has a good transparency, a hightemperature resistance, weather resistance, insulation and stronghydrophobic, which all make the silicone material be the ideal choicefor the LED packaging material.

However, there are technical defects when using the above two kinds ofmaterials for LED packaging materials: the epoxy resin itself hashygroscopicity, easy aging, poor heat resistance, and being easily tochange color under high temperature and short-wave light, large internalstress while curing and other shortcomings, these adverse factors willgreatly affect and shorten the service life of a LED devices; and thesilicone material itself does not have strong mechanical strength andhigh thermal expansion. Obviously, the conventional LED packagingmaterials, while applying these two materials for manufacture, theseadverse factors will have a more serious impact on the performance of aLED packaging materials.

SUMMARY OF THE INVENTION

An embodiment of the present invention provides a new light-emittingdiode (LED) packaging material, which is formed by compounding thegraphene with the silane or the epoxy resin, to improve the defects ofmanufacturing the LED packaging material of the single silane or theepoxy resin, with the help of the properties of graphene, so as toimprove the performance of the LED packaging material.

In the first aspect, the present invention provides a LED packagingmaterial of a first embodiment, the LED packaging material comprisesfollowing raw materials in percentage by weight: a curing agent is10%-40%, a graphene is 0.05%-1%, an epoxy resin is 40%-60%, and anaccelerating agent is 0.5%-2%.

The curing agent is selected from the group consisting of one or more ofmethyltetrahydrophthalic anhydride, divinyltriamine,aminoethylpiperazine, 1,2-diaminocyclohexane, tetraethylenepentamine,bis methylaminopropylamine, dihexyltriamine,methylenebis-phenylenediamine.

The graphene adds hydroxyl groups and/or carboxyl groups to a surface ofthe graphene by a surface modification.

The accelerating agent is for promoting mutual dispersion among the rawmaterials or for promoting mutual dissolution among the raw materialsand for promoting the mixing between the graphene and the epoxy resin.

In the second aspect, the present invention provides a manufacturingmethod of a LED packaging material of a first embodiment, whichcomprises:

a curing agent and a graphene with preset doses are provided, and thecuring agent and graphene are fully mixed.

An epoxy resin and an accelerating agent with preset doses are provided,and added into a mixed solution of the graphene and the curing agent.

The mixed solution of the graphene and the curing agent are fully mixedby ultrasonic to form the LED packaging material formed by compoundingthe graphene and the epoxy resin.

The curing agent is selected from the group consisting of one or more ofmethyltetrahydrophthalic anhydride, divinyltriamine,aminoethylpiperazine, 1,2-diaminocyclohexane, tetraethylenepentamine,bis methylaminopropylamine, dihexyltriamine,methylenebis-phenylenediamine. The graphene adds hydroxyl groups and/orcarboxyl groups to a surface of the graphene by a surface modification.The accelerating agent is for promoting mutual dispersion among the rawmaterials or for promoting mutual dissolution among the raw materialsand for promoting the mixing between the graphene and the epoxy resin.

In the mixed solution constituted of the curing agent, the graphene, theepoxy resin and the accelerating agent. A weight percentage of eachcomponent is as follows: the curing agent is 10%-40%, the graphene is0.05%-1%, the epoxy resin is 40%-60%, and the accelerating agent is0.5%-2%.

An operation method for the step of fully mixing the mixed solution ofthe graphene and the curing agent is as follows: an ultrasonic disperseris used to perform an ultrasonic process to a mixture of the curingagent and the graphene. A power of the ultrasonic 500 W-900 W and aduration is 3-5 hours.

Before the step of fully mixing the mixed solution of the graphene andthe curing agent by ultrasonic, the manufacturing method furthercomprises: the mixed solution of the graphene and the curing agent arestirred by a glass rod, so that the components in the mixed solution areuniformly distributed.

After the step of fully mixing the mixed solution of the graphene andthe curing agent by ultrasonic, the manufacturing method furthercomprises: the mixed solution fully mixed by ultrasonic is placed in avacuum oven and is baked at 60-80° C. for 1 hour, to remove air bubblesin the mixed solution.

In the third aspect, the present invention provides a LED packagingmaterial of a second embodiment, the LED packaging material ismanufactured by a silane, a control agent, a basic ion exchange resins,and a graphene. A mass percentage of the basic ion exchange resin is5%-10%. A mass percentage of the graphene is 0.5%-2%. A molar ratio ofthe silane and the control agent is 1:0.3-1:1.

The control agent comprises terminal hydroxyl groups; and the basic ionexchange resin is a basic anion exchange resin or a basic cationexchange resin.

In the fourth aspect, the present invention provides a manufacturingmethod of a LED packaging material of a second embodiment, whichcomprises:

a silane, a control agent, a basic ion exchange resin and a graphenewith preset doses are mixed and heated, to form a packaging materialsample.

Impurities in the packaging material sample are removed, to obtain theLED packaging material.

In the step of mixing and heating a silane, a control agent, a basic ionexchange resin and a graphene with preset doses, a heating temperatureis 30-80° C. and a heating duration is 5-20 hours.

The impurities in the packaging material sample comprises a residual thebasic ion exchange resin left by insufficient reaction, and the residualbasic ion exchange resin can be removed by filtration.

The impurities in the packaging material sample further comprise a lowboiling point solvent, and the low boiling point solvent can be removedby depressurization.

A mass percentage of the ion exchange resin is 5%40%. A mass percentageof the graphene is 0.5%-2%. A molar ratio of the silane and the controlagent is 1:0.3-1:1. The control agent comprises terminal hydroxylgroups. The basic ion exchange resin is a basic anion exchange resin ora basic cation exchange resin.

The LED packaging material provided by the embodiment of the presentinvention is formed by compounding the graphene with the silane or theepoxy resin, to improve the defects of manufacturing the LED packagingmaterial of the single silane or the epoxy resin, with the help of theproperties of graphene, so as to improve the performance of the LEDpackaging material.

BRIEF DESCRIPTION OF THE DRAWINGS

In order to describe the technical solutions in the embodiments of thepresent invention or in the conventional art more clearly, theaccompanying drawings required for describing the embodiments or theconventional art are briefly introduced. Apparently, the accompanyingdrawings in the following description only show some embodiments of thepresent invention. For those skilled in the art, other drawings may beobtained based on these drawings without any creative work.

FIG. 1 is a flow chart of a manufacturing method of the LED packagingmaterial of a first embodiment according to the present invention.

FIG. 2 is a flow chart of a manufacturing method of the LED packagingmaterial of a second embodiment according to the present invention.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

The technical solutions in the embodiments of the present invention areclearly and completely described below with reference to theaccompanying drawings in the embodiments of the present invention.Obviously, the described embodiments are only some embodiments of thepresent invention, rather than all of the embodiments. All otherembodiments obtained by persons of ordinary skill in the art based onthe embodiments of the present invention without creative efforts shallfall within the protection scope of the present invention.

In addition, the following description of the embodiments is given withreference to the appended drawings, for the purpose of illustratingcertain embodiments in which the invention may be practiced. Directionalterms such as “up”, “down”, “front”, “back”, “left”, “right”, “inside”,“outside”, “side” are used to refer to the attached drawings. Therefore,the directional terms are used for better and more clearly illustratingand understanding the present invention, rather than indicating orimplying that the device or element must have a specific orientation,manufactured and operated by a specific orientation, and thus could notbe understood as a limitation of the present invention.

In the description of the present invention, it should be noted that theterms “mounted,” “connected,” and “connected” should be broadlyunderstood unless the context clearly indicates. For example, maybe afixed connection, a removable connection, an integral connection, amechanical connection, a direct connection, and an indirectly connectionthrough an intermediary, an internal communication between the twoelements. For those skilled in the art, the specific meanings of theabove terms in the present invention may be understood based on specificcases.

In addition, in the description of the present invention, unless withspecial description, the meaning of “plural” is two or more. When theterm “process” appears in the present specification, the term “process”is used to mean not only an independent process, but also an expectedeffect that can be expected from the process unless clearlydistinguished from other processes. The numerical range denoted by “-”in the present specification means a range including the numericalvalues described before and after “-” as the minimum value and themaximum value, respectively. In the drawings, elements that are similarin structure or the same are denoted by the same reference numerals.

The present invention provides a light-emitting diode (LED) packagingmaterial and the manufacturing method of the same, the LED packagingmaterial is formed by compounding the graphene with the silane or theepoxy resin, to improve the defects of manufacturing the LED packagingmaterial of the single silane or the epoxy resin, with the help of theproperties of graphene, so as to improve the performance of the LEDpackaging material. A detailed description is as below.

In a LED packaging material of a first embodiment of the presentinvention, the LED packaging material comprises following raw materialsin percentage by weight: a curing agent is 10%-40%, a graphene is0.05%-1%, an epoxy resin is 40%-60%, and an accelerating agent is0.5%-2%.

In the embodiment, the curing agent is selected from the groupconsisting of one or more of methyltetrahydrophthalic anhydride,divinyltriamine, aminoethylpiperazine, 1,2-diaminocyclohexane,tetraethylenepentamine, bis methylaminopropylamine, dihexyltriamine,methylenebis-phenylenediamine.

In the embodiment, the graphene adds hydroxyl groups and/or carboxylgroups to a surface of the graphene by a surface modification.

In the embodiment, the accelerating agent is for promoting mutualdispersion among the raw materials or for promoting mutual dissolutionamong the raw materials and for promoting the mixing between thegraphene and the epoxy resin. The type of the accelerating agent is notspecifically limited in the present invention as long as it is possibleto accelerate sufficient mixing between the graphene and the epoxyresin.

The LED packaging material provided by the embodiment uses the curingagent and accelerating agent to accelerate for compounding the grapheneand the epoxy resin to form the LED packaging material, to overcome theproblem of hygroscopicity, easy aging, poor heat resistance, and beingeasily to change color under high temperature and short-wave light,large internal stress while curing and etc., making the thermalconductivity, environmental stability, mechanical properties, thermalstability and so on of the LED packaging material highly raised.

Please refer to FIG. 1, which is a flow chart of a manufacturing methodof the LED packaging material of a first embodiment according to thepresent invention. In the embodiment, the manufacturing method of theLED packaging material comprises at least below steps:

Step 1, a curing agent and a graphene with preset doses are provided,and the curing agent and graphene are fully mixed.

In an embodiment of the present invention, the graphene is in a powderform, so as to facilitate thorough mixing with the curing agent. Inaddition, the graphene may be surface-modified before being mixed withthe curing agent and groups such as hydroxyl groups and/or carboxylgroups may be added to the surface of the graphene so as to improve theperformance of the graphene.

In one embodiment of the present invention, the curing agent is selectedfrom the group consisting of one or more of methyltetrahydrophthalicanhydride, divinyltriamine, aminoethylpiperazine,1,2-diaminocyclohexane, tetraethylenepentamine, bismethylaminopropylamine, dihexyltriamine, methylenebis-phenylenediamineand so on. The type of the curing agent is not specifically definedherein.

In one embodiment of the present invention, an operation method for thestep of fully mixing the mixed solution of the graphene and the curingagent is as follows: an ultrasonic disperser is used to perform anultrasonic process to a mixture of the curing agent and the graphene. Apower of the ultrasonic 500 W-900 W and a duration is 3-5 hours.

Step 2, an epoxy resin and an accelerating agent with preset doses areprovided, and added into a mixed solution of the graphene and the curingagent, meanwhile, the mixed solution comprises the curing agent, thegraphene, the epoxy resin, and the accelerating agent.

In one embodiment of the present invention, the epoxy resin is the sameas the epoxy resin commonly used in the conventional LED packagingmaterials and will not be described in detail herein.

In one embodiment of the present invention, the accelerating agent isfor promoting mutual dispersion among the raw materials or for promotingmutual dissolution among the raw materials and for promoting the mixingbetween the graphene and the epoxy resin. The type of the acceleratingagent is not specifically limited in the present invention as long as itis possible to accelerate sufficient mixing between the graphene and theepoxy resin.

In one embodiment of the present invention, in the mixed solutionconstituted of the curing agent, the graphene, the epoxy resin and theaccelerating agent, a weight percentage of each component is as follows:the curing agent is 10%-40%, the graphene is 0.05%-1%, the epoxy resinis 40%-60%, and the accelerating agent is 0.5%-2%.

Step 3, the mixed solution of the graphene and the curing agent arefully mixed by ultrasonic to form the LED packaging material formed bycompounding the graphene and the epoxy resin.

In one embodiment of the present invention, before the step of fullymixing the mixed solution of the graphene and the curing agent byultrasonic, the manufacturing method further comprises: the mixedsolution of the graphene and the curing agent are stirred by a glassrod, so that the components in the mixed solution are uniformlydistributed. After the components in the mixed solution are uniformlystirred by the glass rod, the components are sufficiently mixed by theultrasonic method. In one embodiment of the present invention, theduration of the stirring by the glass rod is 20 minutes and the durationof mixing by ultrasonic usually takes 1 hour.

In one embodiment of the present invention, after the step of fullymixing the mixed solution of the graphene and the curing agent byultrasonic, the manufacturing method further comprises: the mixedsolution fully mixed by ultrasonic is placed in a vacuum oven and isbaked at 60-80° C. for 1 hour, to remove air bubbles in the mixedsolution. After the LED packaging material is formed by the mixedsolution of the graphene and the curing agent, the residuallow-boiling-point solvent is volatilized into a gaseous state to formthe bubbles. Therefore, the gaseous state solvent which is volatilized(the bubbles) can be removed; the bubbles in the mixed solution can beexcluded.

The manufacturing method of the LED packaging material of the embodimentuse the ultrasonic method to fully mix the curing agent, theaccelerating agent, the graphene, and the epoxy resin, to overcome theproblem of hygroscopicity, easy aging, poor heat resistance, and beingeasily to change color under high temperature and short-wave light,large internal stress while curing and etc., making the thermalconductivity, environmental stability, mechanical properties, thermalstability and so on of the LED packaging material highly raised.

In the LED packaging material of the second embodiment of the presentinvention, the LED packaging material is manufactured by a silane, acontrol agent, a basic ion exchange resins, and a graphene. A masspercentage of the basic ion exchange resin is 5%-10%, a mass percentageof the graphene is 0.5%-2%, a molar ratio of the silane, and the controlagent is 1:0.3-1:1.

In the embodiment of the present invention, the type of the silane canbe methyltrichlorosilane, dimethyldichlorosilane, phenyltrichlorosilane, diphenyl dichlorosilane and other organic siliconmonomer, but also other groups substituted silicone monomer, Such asalkoxysilanes and the like. In the embodiment of the present invention,the type of the silane is not specifically limited.

In an embodiment of the present invention, the specific type of thecontrol agent is not limited as long as it has a terminal hydroxylgroup, for example, a terminal hydroxyl-terminated polydimethylsiloxaneand the like.

In an embodiment of the present invention, the specific type of thebasic ion exchange resin is not limited, and may be a basic anionexchange resin or a basic cation exchange resin.

The LED packaging material provided by the embodiment uses the controlagent and the basic ion exchange resin to accelerate compounding thegraphene and the silane, to form the LED packaging material, to overcomethe adverse factors such as low weak mechanical strength, high thermalexpansion and so on, existed while forming the LED packaging materialwith only silane, as the LED packaging material, these adverse factorswill become a more serious problem. Hence, the LED packaging material ofthe present invention uses the control agent and the basic ion exchangeresin to accelerate compounding the graphene and the silane, to form theLED packaging material, making the thermal conductivity, environmentalstability, mechanical properties, and thermal stability and so on of theLED packaging material highly raised.

Please refer to FIG. 2, which is a flow chart of a manufacturing methodof the LED packaging material of a second embodiment according to thepresent invention, which can manufacture the LED packaging material ofthe second embodiment. In the embodiment, the manufacturing method ofthe LED packaging material comprises at least below steps:

Step 21, a silane, a control agent, a basic ion exchange resin and agraphene with preset doses are mixed and heated, to form a packagingmaterial sample.

In the embodiment of the present invention, the type of the silane canbe methyltrichlorosilane, dimethyldichlorosilane, phenyltrichlorosilane, diphenyl dichlorosilane and other organic siliconmonomer, but also other groups substituted silicone monomer, such asalkoxysilanes and the like. In the embodiment of the present invention,the type of the silane is not specifically limited.

In an embodiment of the present invention, the specific type of thecontrol agent is not limited as long as it has a terminal hydroxylgroup, for example, a terminal hydroxyl-terminated polydimethylsiloxaneand the like.

In an embodiment of the present invention, a mass percentage of thebasic ion exchange resin is 5%-10%, a mass percentage of the graphene is0.5%-2%, and a molar ratio of the silane and the control agent is1:0.3-1:1.

In an embodiment of the present invention, in the step of mixing andheating a silane, a control agent, a basic ion exchange resin and agraphene with preset doses, a heating temperature is 30-80° C. and aheating duration is 5-20 hours, to form the packaging material sample.

Step 22, impurities in the packaging material sample are removed, toobtain the LED packaging material.

In an embodiment of the present invention, the impurities in thepackaging material sample comprises a residual the basic ion exchangeresin left by insufficient reaction, and hence, the residual basic ionexchange resin can be removed by filtration.

In an embodiment of the present invention, the impurities in thepackaging material sample further comprises a low boiling point solvent,such as alkaline ion exchange resin solvent, hence, the low boilingpoint solvent can be removed by depressurization. The principle is asfollows: the low boiling point of the encapsulating material sample iseasily volatilized into a gaseous state, and then the solvent with a lowboiling point can be removed by depressurizing it, to remove the lowboiling point solvent.

It can be understood that, when the impurities in the sample of thepackaging material sample include both the residual basic ion exchangeresin left by insufficient reaction and the low boiling point solvent asdescribed above, the two impurities may be sequentially removed byfiltration and depressurization.

The manufacturing method of a LED packaging material of the embodimentuses the basic ion exchange resin and the control agent to acceleratecompounding the graphene and the silane, to form the LED packagingmaterial, to overcome the problem of low weak mechanical strength, highthermal expansion and so on, existed while forming the LED packagingmaterial with only silane, hence, making the thermal conductivity,environmental stability, mechanical properties, thermal stability and soon of the LED packaging material highly raised.

In the description of the present specification, the description withreference to the terms “one embodiment,” “some embodiments,” “anexample,” “a specific example,” “some examples,” and the like means aparticular feature described in connection with the embodiment orexample. The structures, materials, or characteristics are included inat least one embodiment or example of the present invention. In thisspecification, the schematic representation of the above terms does notnecessarily refer to the same embodiment or example. Furthermore, theparticular features, structures, materials, or characteristics describedmay be combined in any suitable manner in any one or more embodiments orexamples.

The LED packaging material and the liquid crystal display panel providedby the embodiments of the present disclosure are described in detailabove. Specific examples are used herein to describe the principle andimplementation manners of the present disclosure. The description of theabove embodiments is merely used to help understand the presentdisclosure and its core concept; meanwhile, those skilled in the art maymake changes to the specific implementing manners and the applicationscope according to the concept of the present invention. In view of theabove, the contents of the description should not be construed aslimitations of the invention.

What is claimed is:
 1. A method for manufacturing a light-emitting diode(LED) packaging material, comprising the following steps: mixinggraphene with a curing agent at a predetermined ratio to form a firstmixed solution including a mixture of graphene and the curing agent;providing epoxy resin and an accelerating agent with a predeterminedratio, and adding the epoxy resin and the accelerating agent into thefirst mixed solution of graphene and the curing agent to form a secondmixed solution, which comprises the mixture of graphene and the curingagent that is added with epoxy resin and the accelerating agent; andsubjecting the second mixed solution to an ultrasonic process to form amaterial of a fully-mixed combination of graphene and epoxy resin,wherein the first mixed solution is formed by mixing graphene and thecuring agent before epoxy resin is added in the first mixed solution. 2.The method according to claim 1, wherein the curing agent is selectedfrom a group consisting of one or more of methyltetrahydrophthalicanhydride, divinyltriamine, aminoethylpiperazine,1,2-diaminocyclohexane, tetraethylenepentamine, bismethylaminopropylamine, dihexyltriamine, methylenebis-phenylenediamine;wherein graphene is subjected to surface modification to add hydroxylgroups and/or carboxyl groups to a surface of graphene; wherein theaccelerating agent promotes mutual dispersion or mutual dissolutionamong ingredients of the second mixed solution so as to enhance mixtureof graphene and epoxy resin included in the second mixed solution. 3.The method according to claim 1, wherein in the second mixed solutionformed of the curing agent, graphene, epoxy resin and the acceleratingagent, a weight percentage of each of ingredient components of thesecond mixed solution is as follows: the curing agent is 10%-40%;graphene is 0.05%4%; epoxy resin is 40%-60%; and the accelerating agentis 0.5%-2%.
 4. The method according to claim 1, wherein an operation ofmixing graphene and the curing agent comprises operating an ultrasonicdisperser to perform an ultrasonic process to the mixture of grapheneand the curing agent, wherein a power of the ultrasonic 500 W-900 W anda duration is 3-5 hours.
 5. The method according to claim 1, wherein thesecond mixed solution that comprises the mixture of graphene and thecuring agent added that is added with epoxy resin and the acceleratingagent is subjected to stirring with a glass rod to have ingredientcomponents of the second mixed solution uniformly distributed before theultrasonic process is carried out on the second mixed solution.
 6. Themethod according to claim 1, wherein after the ultrasonic processcarried out on the second mixed solution, an operation is carried out bysubjecting the second mixed solution to baking at 60-80° C. for 1 hourin a vacuum oven in order to remove air bubbles in the second mixedsolution.
 7. The method according to claim 3, wherein after theultrasonic process carried out on the second mixed solution, anoperation is carried out by subjecting the second mixed solution tobaking at 60-80° C. for 1 hour in a vacuum oven in order to remove airbubbles in the second mixed solution.
 8. The method according to claim5, wherein after the ultrasonic process carried out on the second mixedsolution, an operation is carried out by subjecting the second mixedsolution to baking at 60-80° C. for 1 hour in a vacuum oven in order toremove air bubbles in the second mixed solution.